Abstract: The extraction of zinc and iron with N263 from chloride solution was studied. The effects of oscillation time, extractant concentration, modifier concentration, phase ratio(O/A), and hydrochloric acid concentration on the extraction rate of zinc and iron were investigated. The results showedthe extraction rate of Zn²⁺, Fe²⁺ and Fe³⁺ were 90.97%, 0.79% and 75.85%, respectively, and the separation coefficient of β_{Zn²⁺/Fe²⁺}and β_{Zn²⁺/Fe³⁺} were 1 260 and 3.21, respectively, under the conditions of extractant composition of 20% N263+20% n-hexanol+60% 260^# solvent oil, phase ratio(O/A) of 1 GA6FA 1, oscillation time of 5 min, 25 ℃. Meanwhile, the concentration of zinc in the aqueous phasedecreased from 9.61 g/L to 0.36 g/L by two-stage countercurrent extraction. The stripping rate of Zn²⁺ was 41.86% and more than 97% of Fe³⁺ was stripped with 0.5 mol/L sulfuric acid. Additionally, the mechanism of extraction of metal ions by N263 is anion exchange reaction. The extraction equilibrium isotherms of zinc and iron were plotted, and the thermodynamic functions of the extraction reaction were calculated. The results indicated that the extraction of Zn²⁺ by N263 is exothermic, and the extraction of Fe³⁺ is endothermic. The extraction of Zn²⁺ and Fe³⁺ can proceed spontaneously at room temperature.